Ultra‐Fast and Economical Pre‐Breakdown Electrochemical Synthesis of Intrinsically Conductive Polymer Suspension for Production of Safe Lithium‐Ion Batteries

We report a novel pre‐breakdown electrochemical synthesis method for producing polyNiMeOSalen suspensions with exceptional scalability and economic viability. Operating at ultra‐high current density (1 A cm −2 ), this method achieves 83% yield and produces nanoscale particles (~30 nm) with superior electrochemical performance. The resulting P‐polyNiMeOSalen demonstrates 1.7 times higher rate capability than conventional electrochemically synthesized materials, attributed to increased surface area and enhanced non‐Faradaic contributions. Techno‐economic analysis reveals remarkable commercial potential with production costs of circa $1500/kg (significantly lower than competing materials), rapid payback period (1.17 years), and high internal rate of return (49.5%). Despite the presence of impurities, P‐polyNiMeOSalen, when employed as a protective layer in composite cathodes with NMC532, demonstrates negligible impact on the Coulombic efficiency of NMC532, achieving 99.3% by the fifth cycle. Furthermore, P‐polyNiMeOSalen exhibits comparable protective properties to E‐polyNiMeOSalen upon overcharge of NMC532 to 8 V. This scalable synthesis represents a paradigm shift toward the economically viable production of protective coatings for next‐generation lithium‐ion battery safety systems.